CN114427072A - Alloy on-line treatment method, alloy and application - Google Patents
Alloy on-line treatment method, alloy and application Download PDFInfo
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- CN114427072A CN114427072A CN202011096484.6A CN202011096484A CN114427072A CN 114427072 A CN114427072 A CN 114427072A CN 202011096484 A CN202011096484 A CN 202011096484A CN 114427072 A CN114427072 A CN 114427072A
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
- C23C8/16—Oxidising using oxygen-containing compounds, e.g. water, carbon dioxide
- C23C8/18—Oxidising of ferrous surfaces
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D7/00—Modifying the physical properties of iron or steel by deformation
- C21D7/02—Modifying the physical properties of iron or steel by deformation by cold working
- C21D7/04—Modifying the physical properties of iron or steel by deformation by cold working of the surface
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses an alloy on-line treatment method, an alloy and application. The method comprises the following steps: carrying out extrusion grinding treatment on the surface of the alloy; then, oxidation treatment is performed in a mixed gas atmosphere of hydrogen and water vapor. The abrasive material for extrusion grinding treatment is formed by mixing abrasive particles and a viscous liquid carrier. The abrasive particles are selected from one or more of tungsten oxide, cerium oxide, chromium oxide, aluminum oxide, silicon carbide, boron carbide and diamond; the abrasive grains have a grain size of 40-1000 meshes and account for 10-80 wt% of the total weight of the abrasive. The viscous liquid carrier is one or more selected from vaseline, paraffin, turpentine and oleic acid; the viscous liquid carrier accounts for 20-90 wt% of the total weight of the abrasive. The surface of the alloy is subjected to extrusion grinding treatment, so that a brittle layer on the surface is removed; the alloy is also oxidized to form a very compact oxide layer on the surface of the alloy. Effectively improves the oxidation resistance, coking resistance and anti-carburizing capability of the alloy.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to an alloy on-line treatment method, an alloy and application.
Background
Ethylene, propylene, butadiene and benzene, toluene, xylene are all basic raw materials for the petrochemical industry. Ethylene yield, production scale and technology mark a state of the petrochemical industry. The current method for producing ethylene is mainly based on the tubular furnace cracking technology, and is widely applied worldwide.
After hydrocarbon steam cracking for a period of time, a layer of thick coke is deposited on the inner surface of a furnace tube of a cracking furnace radiation section, the thermal resistance of the furnace tube is increased by a coke layer, the heat transfer coefficient is reduced, when the coke layer reaches a certain thickness, the cracking furnace tube must stop producing, and air-steam combined coking is adopted. In order to further remove coke, pure air at 850 ℃ for 20 hours is often burnt in the later stage of burning, and the pure air without water vapor causes excessive oxidation of the cracking furnace tube at high temperature, so that the matrix of the furnace tube is peeled off or the matrix oxide is volatilized, for example, very thick Cr is generated on the inner surface2O3Oxide film, excessive thickness of Cr2O3The oxide film is liable to peel off due to a large difference in thermal expansion coefficient between the oxide film and the furnace tube base, and excessive oxidation causes Cr on the base surface2O3Will be transformed into CrO3The gas is volatilized. Matrix Cr2O3The areas left after the oxide film is peeled off or volatilized are areas rich in Fe and Ni elements which are the key factors causing catalytic coking, so that local severe coking and carburization can be caused by excessive oxidation, and the service life of the hydrocarbon cracking furnace tube can be greatly reduced.
The oxidation and coking prevention of the inner surface of the cracking furnace tube is generally realized by coating the inner surface of the furnace tube with a metallurgical coatingLayer, mainly forming one or more metallurgical coatings with good mechanical property and thermal stability on the inner surface of the furnace tube by plasma spraying, hot sputtering, high-temperature sintering and other methods, such as Al2O3、Cr2O3、SiO2And the like.
Chinese patent CN 1580316A embeds a furnace tube into a device filled with a co-permeation agent, then carries out temperature-changing heating, constant temperature and cooling heat treatment on the furnace tube, the whole process is protected by argon, finally a layer of metal inert material is formed on the inner surface of the furnace tube, and small test results show that the coke content is reduced by 50%. The method has the disadvantages that the preparation process of the coating is complex, and the coating and the substrate are easy to peel off because a transition layer is not arranged between the coating and the substrate.
In the US patent US 6537388, Cr and Si compounds are filled in a furnace tube, Cr and Si elements are diffused into the metal of a substrate furnace tube to form a Cr-Si bottom layer after passivation treatment, then Si and Al compounds are sprayed on the Cr-Si bottom layer by adopting a hot sputtering method, and an Si-Al outer layer is formed after heat treatment. The method has the defects of complex coating preparation process and certain damage effect on the furnace tube matrix.
U.S. Pat. No. 4, 6585864 discloses a coke-inhibiting technique for a coat-alloy ethylene furnace tube, which comprises depositing NiCrAlY coating material on a substrate alloy by magnetron sputtering, and heat treating to form a coating comprising a diffusion barrier layer, a enrichment pool layer, and alpha-Al2O3And (3) a composite coating of an anti-coking layer. The method has the disadvantages of complex coating preparation process, multiple steps and high cost.
U.S. Pat. No. 4, 6423415 discloses a mixture of K and K in a certain molar ratio2O、SiO2、Al2O3、ZnO、MgO、Co3O4、Na2O、ZrO2Spraying inorganic substances onto the furnace tube at high temperature2、N2And sintering in a water vapor atmosphere to form the glass coating. The method has the defects that the expansion coefficients of the inorganic coating and the furnace tube matrix are greatly different, and the service life of the coating is influenced after the temperature of production and decoking is repeatedly changed.
U.S. Pat. No. 4, 5648178 discloses a method for preparing HP-Method for 50 Cr coating of metal, CrCl2The powder is prepared into a coating with certain viscosity, and the coating is coated on the metal surface and then is subjected to pure H2Heat treating in atmosphere to form firm Cr coating, dry carbonizing the Cr coating with propane-containing hydrogen to form carbon-rich binding layer, and bonding with N2Treating to form CrN filled cracks, and treating with steam to form thin Cr2O3And the layer is covered on the surface of the chromium layer. Cr formed by the method2O3The coating easily peels off.
The coating in the patent covers Fe and Ni elements with catalytic coking activity on the inner wall of the furnace tube, and can prevent oxygen elements and carbon elements in the atmosphere from entering a furnace tube substrate, but the coating process is complex, high in cost and limited in service life, and the coating process has great influence on the component distribution and the tissue structure of the whole furnace tube, so that the coating technology is not adopted by ethylene manufacturers in a large scale.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an alloy on-line treatment method, an alloy and application. The invention does not improve the oxidation resistance, coking resistance and anti-carburizing capability of the cracking furnace tube alloy in a coating mode, but finely adjusts the contents of Si and Mn elements in the components of the alloy, and basically does not influence the mechanical property and welding property of the alloy; the surface of the alloy is subjected to extrusion grinding treatment, and a brittle layer on the surface is removed; the alloy is also subjected to high-temperature hydrogen-steam pre-oxidation treatment, so that a very compact oxide layer is formed on the surface of the alloy. Effectively improves the oxidation resistance, coking resistance and anti-carburizing capability of the alloy.
The invention aims to provide an alloy on-line treatment method.
The method comprises the following steps:
carrying out extrusion grinding treatment on the surface of the alloy; then, oxidation treatment is performed in a mixed gas atmosphere of hydrogen and water vapor.
Oxidation treatment with water vapor in the atmosphere in H2When present, H2The more, reaction H2O＝0.5O2+H2Equilibrium of (a) is shifted to the left, O2The less, the less oxidizing.
In a preferred embodiment of the present invention,
the abrasive material for extrusion grinding treatment is formed by mixing abrasive particles and a viscous liquid carrier.
In a preferred embodiment of the present invention,
the abrasive particles are selected from one or more of tungsten oxide, cerium oxide, chromium oxide, aluminum oxide, silicon carbide, boron carbide and diamond;
the abrasive grains have a grain size of 40-1000 meshes and account for 10-80 wt% of the total weight of the abrasive.
In a preferred embodiment of the present invention,
the viscous liquid carrier is one or more selected from vaseline, paraffin, turpentine and oleic acid;
the viscous liquid carrier accounts for 20-90 wt% of the total weight of the abrasive.
In a preferred embodiment of the present invention,
the pressure of extrusion grinding is 0.5MPa-15 MPa; the extrusion grinding time is 5-3600 seconds.
In a preferred embodiment of the present invention,
the volume of the water vapor is 20 to 70 percent of the total volume of the mixed gas;
in a preferred embodiment of the present invention,
the oxidation treatment temperature is 800-1100 ℃; the oxidation treatment time is 5 to 50 hours.
The second purpose of the invention is to provide an alloy treated by the method.
Based on the total weight of the alloy as 100 percent,
the alloy comprises:
1-50% of chromium; preferably 10-40%;
1-50% of nickel; preferably 10-50%;
0.2-3% of manganese; preferably 0.5-3%;
0-3% of silicon; preferably 0.5-3%;
carbon < 0.75%;
0-5% of trace elements and/or trace elements;
the balance being iron;
the trace elements are one or more of niobium, titanium, tungsten, aluminum and rare earth elements,
the trace elements are sulfur or/and phosphorus.
In a preferred embodiment of the present invention,
the mass percentage of Si and Mn in the alloy meets the following conditions:
[Mn]≥1.0
[Si]≥1.0
the invention also aims to provide the application of the alloy in cracking equipment.
The following technical scheme can be specifically adopted in the application:
the oxidation-resistant, coking-resistant and carbonization-resistant alloy comprises the following contents:
(1) the alloy comprises the following components in percentage by weight: 1-50% of chromium, 1-50% of nickel, 0.2-3% of manganese, 0-3% of silicon, 0.75% of carbon, 0-5% of trace elements and/or trace elements and the balance of iron; the trace elements are one or more of niobium, titanium, tungsten, aluminum and rare earth elements, and the trace elements are sulfur or/and phosphorus.
(2) The mass percentage of Si and Mn in the alloy meets the following conditions:
[Mn]≥1.0
[Si]≥1.0
(3) the surface of the alloy is subjected to extrusion grinding treatment, and the grinding material is formed by mixing abrasive particles and a viscous liquid carrier according to a certain proportion. The abrasive particles are selected from one or more of tungsten oxide, cerium oxide, chromium oxide, aluminum oxide, silicon carbide, boron carbide and diamond. The grain size of the abrasive particles is 40-1000 meshes, and the weight percentage of the abrasive particles is 10-80%. The viscous liquid carrier is selected from one or more of vaseline, paraffin, oleum Terebinthinae, and oleic acid. The weight percentage of the viscous liquid carrier is 20-90%. The pressure of the extrusion grinding is 0.5MPa-15 MPa. The extrusion grinding time is 5-3600 seconds.
(4) And treating the alloy after extrusion grinding for 5-50 hours in an oxidizing mixed gas atmosphere at 800-1100 ℃, wherein the oxidizing mixed gas comprises hydrogen and water vapor, and the volume of the water vapor is 20-70% of the total volume of the oxidizing mixed gas. Because of the high water vapor content, the step is carried out on line after the alloy furnace tube is installed in the cracking furnace.
The cracking furnace tube alloy is oxidized by water vapor in the cracking atmosphere in the service process, and Cr is formed on the surface2O3Mainly an oxide film. The alloy of the invention increases the contents of Si and Mn, and mainly aims at increasing MnO and SiO in an alloy oxide layer2To reduce Cr content2O3Content because Si forms SiO during oxidation2A layer which, like a barrier, prevents part of the Cr element from migrating to the surface layer and thus does not form excessive Cr2O3，Cr2O3Is not very protective since it is converted to CrO above 950 ℃3The gas is volatilized. The MnO content in the alloy oxide film of the invention is increased and then is mixed with Cr2O3Form more stable MnCr2O4Or Mn1.5Cr1.5O4。
Under the action of extrusion and grinding, the brittle layer and the microscopic defects on the surface of the alloy are removed in a large amount, the organization structure of the inner surface of the furnace tube is more compact, the grains are refined, the grain size of an oxide film formed on the surface of the furnace tube is smaller and more compact, the oxide film is not easy to peel off, and the protection performance is stronger.
The hydrogen-water vapor provided by the invention has the advantages that the oxidation treatment of the alloy is carried out by using the hydrogen-water vapor, compared with the oxygen partial pressure of the pyrolysis gas-water vapor atmosphere in the pyrolysis process, the oxidation rate is slower, the particle size of the formed oxidation film is smaller, the oxidation layer is firmer, and the service life is longer.
Drawings
FIG. 1 is a schematic view of an oxidation experimental apparatus according to the present invention;
FIG. 2 is an oxidation weight gain curve for comparative example 1, comparative example 2, comparative example 3, example 1;
FIG. 3 is a coke weight gain curve for comparative example 1, comparative example 2, comparative example 3, example 1;
FIG. 4 is a graph of the carbonization weight gain of comparative example 1, comparative example 2, comparative example 3, and example 1;
FIG. 5 is an oxidation weight gain curve for comparative example 4, comparative example 5, comparative example 6, example 2;
FIG. 6 is a coke weight gain curve for comparative example 4, comparative example 5, comparative example 6, example 2;
FIG. 7 is a graph of the carbonization weight gain of comparative example 4, comparative example 5, comparative example 6, and example 2;
FIG. 8 is an oxidation weight gain curve for comparative example 7, comparative example 8, comparative example 9, example 3;
FIG. 9 is a coke weight gain curve for comparative example 7, comparative example 8, comparative example 9, example 3;
fig. 10 is a carbonization weight gain curve of comparative example 7, comparative example 8, comparative example 9, and example 3.
Description of reference numerals:
(1) a gas mass flow meter; (2) a peristaltic pump; (3) a preheater; (4) an electric heating furnace; (5) a condenser; (6) a vacuum pump; (7) a wet gas flowmeter.
Detailed Description
While the present invention will be described in detail and with reference to the specific embodiments thereof, it should be understood that the following detailed description is only for illustrative purposes and is not intended to limit the scope of the present invention, as those skilled in the art will appreciate numerous insubstantial modifications and variations therefrom.
The adjustment of the silicon-manganese content described in the examples and comparative examples means that: the contents of silicon and manganese are slightly increased in the smelting process, and other elements and smelting processes do not need to be changed.
Comparative examples 1, 4, 7
The alloy used is common 2520, 2535, 3545 alloy; the surface composition was analyzed by an X-ray energy dispersive spectrometer and the results are shown in Table 1.
Comparative examples 2, 5 and 8
The used alloys are 2520, 2535 and 3545 alloys with the adjusted contents of Si and Mn elements;
the serial numbers are respectively as follows: 2520-1, 2535-1, 3545-1; the surface composition was analyzed by an X-ray energy dispersive spectrometer and the results are shown in Table 1.
Comparative example 3
The content of Si and Mn elements is adjusted by 2520 alloy,
a numerical control linear cutting machine is used for cutting square samples with the size of 5mm multiplied by 3mm, and the wire moving speed of the wire cutting is controlled, so that the surface roughness of each sample is basically consistent. Then the sample was subjected to extrusion grinding treatment under the following conditions:
extruding and grinding: (1) abrasive formulation, 15% alumina (800 mesh) + 35% boron carbide (400 mesh) + 35% paraffin + 15% oleic acid; (2) extrusion grinding pressure, 5 MPa; (3) extrusion milling time, 60 seconds.
Alloy No. 2520-2 was analyzed for its surface composition by X-ray energy dispersive spectroscopy, and the results are shown in Table 1.
Comparative example 6
2535 alloy is adopted to adjust the contents of Si and Mn elements
A numerical control linear cutting machine is used for cutting square samples with the size of 5mm multiplied by 3mm, and the wire moving speed of the wire cutting is controlled, so that the surface roughness of each sample is basically consistent. Then the sample was subjected to extrusion grinding treatment under the following conditions:
extruding and grinding: (1) abrasive formula, 76% boron carbide (1000 mesh), 12% paraffin, 10% oleic acid and 2% turpentine; (2) extrusion grinding pressure, 10 MPa; (3) extrusion milling time, 15 seconds.
Alloy No. 2535-2 was analyzed for its surface composition using an X-ray energy dispersive spectrometer and the results are shown in Table 1.
Comparative example 9
Adjusting the contents of Si and Mn elements by using 3545 alloy;
a numerical control linear cutting machine is used for cutting square samples with the size of 5mm multiplied by 3mm, and the wire moving speed of the wire cutting is controlled, so that the surface roughness of each sample is basically consistent. Then the sample was subjected to extrusion grinding treatment under the following conditions:
extruding and grinding: (1) abrasive formulation, 83% silicon carbide (400 mesh) + 17% petrolatum; (2) extrusion grinding pressure is 2 MPa; (3) extrusion milling time, 500 seconds.
Alloy No. 3545-2 was analyzed for surface composition using an X-ray energy dispersive spectrometer and the results are shown in table 1.
Example 1
The content of Si and Mn elements is adjusted by 2520 alloy,
a numerical control linear cutting machine is used for cutting square samples with the size of 5mm multiplied by 3mm, and the wire moving speed of the wire cutting is controlled, so that the surface roughness of each sample is basically consistent. Then the sample was extrusion-milled and pre-oxidized as follows:
extruding and grinding: (1) abrasive formulation, 15% alumina (800 mesh) + 35% boron carbide (400 mesh) + 35% paraffin + 15% oleic acid; (2) extrusion grinding pressure, 5 MPa; (3) extrusion milling time, 60 seconds.
Oxidation treatment of hydrogen and water vapor: the volume of the water vapor is 30 percent of the total volume of the oxidizing mixed gas, the treatment temperature is 850 ℃, and the treatment time is 20 hours.
Alloy Nos. 2520-3 were analyzed for their surface compositions by X-ray energy dispersive spectrometry, and the results are shown in Table 1.
Example 2
Adjusting the contents of Si and Mn elements by using 2535 alloy;
a numerical control linear cutting machine is used for cutting square samples with the size of 5mm multiplied by 3mm, and the wire moving speed of the wire cutting is controlled, so that the surface roughness of each sample is basically consistent. Then the sample was extrusion-milled and pre-oxidized as follows:
extruding and grinding: (1) abrasive formula, 76% boron carbide (1000 mesh), 12% paraffin, 10% oleic acid and 2% turpentine; (2) extrusion grinding pressure, 10 MPa; (3) extrusion milling time, 15 seconds.
Oxidation treatment of hydrogen and water vapor: the volume of the water vapor is 40 percent of the total volume of the oxidizing mixed gas, the treatment temperature is 900 ℃, and the treatment time is 30 hours.
Alloy No. 2535-3 was analyzed for its surface composition using an X-ray energy dispersive spectrometer and the results are shown in Table 1.
Example 3
Adjusting the contents of Si and Mn elements by using 3545 alloy;
a numerical control linear cutting machine is used for cutting square samples with the size of 5mm multiplied by 3mm, and the wire moving speed of the wire cutting is controlled, so that the surface roughness of each sample is basically consistent. Then the sample was extrusion-milled and pre-oxidized as follows:
extruding and grinding: (1) abrasive formulation, 83% silicon carbide (400 mesh) + 17% petrolatum; (2) extrusion grinding pressure is 2 MPa; (3) extrusion milling time, 500 seconds.
Oxidation treatment of hydrogen and water vapor: the volume of the water vapor is 50 percent of the total volume of the oxidizing mixed gas, the treatment temperature is 1000 ℃, and the treatment time is 40 hours
Alloy No. 3545-3 was analyzed for surface composition using an X-ray energy dispersive spectrometer and the results are shown in table 1.
TABLE 1 chemical composition of alloy (wt%)
Bal in the table indicates the balance.
Oxidation test of test piece
The oxidation experiment of the sample was carried out in the apparatus shown in FIG. 1, with the sample suspended in the constant temperature region of the electric heating furnace. The oxidizing gas was air and the flow rate was 200 ml/min. The temperature rising rate of the electric heating furnace is 10 ℃/min, the temperature is kept constant for 3 hours after the temperature rises to 850 ℃, and finally the temperature is reduced, the temperature reduction rate is about-2 ℃/min, and air is introduced in the whole process. Each sample was oxidized 3 times for the first two 3h, the third 4h, and 10 h. And weighing the mass of the sample before and after each oxidation experiment by using an analytical balance to obtain the oxidation weight gain.
Coking experiment of samples
The coking experiment of the sample was carried out in the apparatus shown in FIG. 1, with the sample suspended in the constant temperature zone of an electric furnace. When a coking experiment is carried out, the coking gas is N2-2％C2H6The temperature is raised to 900 ℃ at the temperature raising rate of 10 ℃/min, the temperature is kept for 4 hours at the temperature lowering rate of-2 ℃/min, the coking gas is always introduced in the temperature raising and keeping process, and the gas flow is 200 ml/min. Each sample is coked for 3 times, the first two times are coked for 3 hours, the third time is coked for 4 hours, and the total time is 10 hours. And weighing the mass of the sample before and after each coking experiment to obtain the coking weight gain.
Carbonization test of test specimens
The sample was carbonized in the apparatus shown in FIG. 1, and the sample was suspended in the constant temperature region of the electric heating furnace. When the carbonization experiment is carried out, the carbonization gas is 98 percent H2-2％CH4The temperature is raised to 1000 ℃ at the heating rate of 10 ℃/min and then kept constant for 10h, the temperature reduction rate is about-2 ℃/min, and the carbonized gas is introduced in the heating and constant temperature processes, wherein the gas flow is 200 ml/min. Each sample was carbonized 4 times for 10h each time for 40 h. Before and after each carbonization experiment, the mass of the sample is weighed, and the surface composition of the sample is analyzed by an X-ray energy dispersion spectrometer after carbonization for 40 hours.
Analysis and characterization of samples
The samples were analyzed for surface element content using an Apollo XP type X-ray Energy Dispersive Spectrometer (EDS) from EDAX. The mass of the sample before and after each coking and carbonization test was weighed with an AA-200 electronic analytical balance of Denver corporation to an accuracy of 0.1 mg.
Comparative example 1, comparative example 2, comparative example 3, example 1
2520 alloy has oxidation weight gain curve, coking weight gain curve and carbonization weight gain curve as shown in fig. 2, 3 and 4, and surface element analysis after carbonization is shown in table 2.
TABLE 22520 carbonized surface elements in percent by mass
The oxidation weight gain curve, the coking weight gain curve and the carbonization weight gain curve of the comparative example 4, the comparative example 5, the comparative example 6 and the example 2 are shown in figures 5, 6 and 7; the surface elemental analysis after carbonization is shown in table 3.
Table 32535 carbonized surface element mass percent content
The oxidation weight gain curve, the coking weight gain curve and the carbonization weight gain curve of the comparative example 7, the comparative example 8, the comparative example 9 and the example 3 are shown in figures 8, 9 and 10; the surface elemental analysis after carbonization is shown in table 4.
Surface element mass percentage content of carbonized table 43545 alloy
By combining all the data, the oxidation resistance, the coking resistance and the carbonization resistance of the alloy provided by the invention are greatly improved compared with the conventional alloy.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. An alloy on-line processing method, characterized in that the method comprises:
carrying out extrusion grinding treatment on the surface of the alloy; then, oxidation treatment is performed in a mixed gas atmosphere of hydrogen and water vapor.
2. The process of claim 1, wherein:
the abrasive material for extrusion grinding treatment is formed by mixing abrasive particles and a viscous liquid carrier.
3. The processing method of claim 2, wherein:
the abrasive particles are selected from one or more of tungsten oxide, cerium oxide, chromium oxide, aluminum oxide, silicon carbide, boron carbide and diamond;
the abrasive grains have a grain size of 40-1000 meshes and account for 10-80 wt% of the total weight of the abrasive.
4. The processing method of claim 2, wherein:
the viscous liquid carrier is one or more selected from vaseline, paraffin, turpentine and oleic acid;
the viscous liquid carrier accounts for 20-90 wt% of the total weight of the abrasive.
5. The process of claim 1, wherein:
the pressure of extrusion grinding is 0.5MPa-15 MPa; the extrusion grinding time is 5-3600 seconds.
6. The process of claim 1, wherein:
the volume of the water vapor is 20-70% of the total volume of the mixed gas.
7. The process of claim 1, wherein:
the oxidation treatment temperature is 800-1100 ℃; the oxidation treatment time is 5 to 50 hours.
8. An alloy treated by the method of any one of claims 1 to 7, wherein:
based on the total weight of the alloy as 100 percent,
the alloy comprises:
0-5% of trace elements and/or trace elements;
the balance being iron;
the trace elements are one or more of niobium, titanium, tungsten, aluminum and rare earth elements,
the trace elements are sulfur or/and phosphorus.
9. The alloy of claim 8, wherein:
the mass percentage of Si and Mn in the alloy meets the following conditions:
[Mn]≥1.0
[Si]≥1.0。
10. use of an alloy according to any one of claims 8 to 9 in a cracking apparatus.
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